Method for efficiently synthesizing trifluoromethyl iodide

A high-efficiency technology of trifluoroiodomethane, which is applied in the field of high-efficiency synthesis of trifluoroiodomethane, can solve the problems of large amount of reaction solvent, expensive raw materials and high cost, and achieves the advantages of reasonable design of process steps, accelerated reaction rate and improved utilization rate. Effect

Active Publication Date: 2018-07-06
DALIAN KELIDE OPTOELECTRONICS MATERIALS CO LTD
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In summary, the existing preparation of CF 3 The method of I has expensive raw materials, high cost, a large amount of reaction solvent, a series of problems such as low product yield, poor selectivity, and low utilization of raw materials

Method used

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  • Method for efficiently synthesizing trifluoromethyl iodide

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Embodiment 1

[0022] 1. Synthetic catalyst: 3.0g KNO 3 and 5g RbNO 3 Dissolve in 500mL of water, add 100g of activated carbon to it, ultrasonically treat for 30min, and let it stand overnight; filter, dry the solid isolate at 100°C for 5h, and then calcinate at 500°C for 2h under a high-purity nitrogen atmosphere to prepare the catalyst.

[0023] 2. Synthesis of CF 3 I

[0024] (1) CF 3 COOH vapor and iodine vapor enter the 500°C reactor at a molar ratio of 1:1, and 100g of catalyst is installed in the reactor to control CF 3 The flow rate of COOH vapor is 20mL / min, CF 3 The reaction time of COOH and iodine is 10min to generate CF 3 I.

[0025] (2) Make the above CF 3 The I gas is passed into the first collector, the second collector, the alkali washing tank, the drier and the adsorber successively to remove H 2 O.CO 2 , HF and other impurities. 80°C water is used for circulation outside the primary collector; the lye in the alkali washing tank is 0.5% NaOH solution; the desiccant...

Embodiment 2

[0027] 1. Synthetic catalyst: 7.0g KNO 3 and 0.7g RbNO 3 Dissolve in 500mL of water, add 100g of graphene to it, sonicate for 30min, and let it stand overnight; filter, dry the solid isolate at 100°C for 5h, and then calcinate at 500°C for 2h under a high-purity nitrogen atmosphere to prepare the catalyst.

[0028] 2. Synthesis of CF 3 I

[0029] (1) CF 3 COOH vapor and iodine vapor enter the 550°C reactor at a molar ratio of 2:1, and the reactor is equipped with 100g of catalyst, and the CF is controlled 3 The flow rate of COOH vapor is 20mL / min, CF 3 The reaction time of COOH and iodine is 10min to generate CF 3 I.

[0030] (2) Make the above CF 3 The I gas is passed into the first collector, the second collector, the alkali washing tank, the drier and the adsorber successively to remove H 2 O.CO 2 , HF and other impurities. 80°C water is used for circulation outside the primary collector; the lye in the alkali washing tank is 0.5% NaOH solution; the desiccant in t...

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Abstract

The invention discloses a method for efficiently synthesizing trifluoromethyl iodide. The method comprises the following steps: reacting CF3COOOH vapor with iodine vapor under the action of a catalystto generate the trifluoromethyl iodide, wherein the catalyst is a catalyst which selects activated carbon or graphene as a carrier and is loaded with 1 to 10 weight percent of KNO3 and 2 to 7 weightpercent of RbNO3; then effectively removing impurities and moisture in CF3I by a NaOH solution, silica gel and a molecular sieve in sequence, thus efficiently collecting high-purity CF3I products. Themethod has the advantages of fast reaction rate, good selectivity, high yield, high reactant utilization and energy conservation; the method is expected to realize industrialized production and meetscurrent market demands.

Description

technical field [0001] The invention relates to a method for efficiently synthesizing trifluoroiodomethane. Background technique [0002] Trifluoroiodomethane (CF 3 I) The greenhouse effect potential value (GWP) is less than 5, and the ozone depletion potential value (ODP) is 0. It has been listed by the United Nations as the main component of the third-generation environmentally friendly refrigerant. In addition to being used as a new type of gas fire extinguishing agent and refrigerant, it also has broad application prospects in other fields such as fluorine-containing intermediates, semiconductor etching, and foaming agents. [0003] CF 3 I literature report CF 3 I synthesis technique is numerous, main method has: [0004] (1) Perfluorocarboxylate pyrolysis method: CF 3 COM (M=Ag, Na, K, Hg, Pb, Ba) and iodine (I 2 ) as raw material, thermally decomposed in a strong polar solvent to prepare CF 3 I, this is also the synthetic method that is proposed to have industri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/04C07C17/363C07C19/16
CPCC07C17/363B01J23/002B01J23/04C07C19/16
Inventor 赵毅赵趫王天源计燕秋张琳石琳刘颖
Owner DALIAN KELIDE OPTOELECTRONICS MATERIALS CO LTD
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